Sample supply means for analysis apparatus



June 1, 1965 A. FERRARI 3,185,235

SAMPLE SUPPLY MEANS FOR ANALYSIS APPARATUS Filed April 5. 1962 INVENTOR.

Awgss F5 @419! A rro /ver United States Patent 3,186,235 SAMPLE SUPPLY MEANS FOR ANALYSIS APPARATUS Andrs Ferrari, Scarsdale, N.Y., assignor to Technicon Instruments Corporation, Chauncey, N.Y., a corporation of New York Filed Apr. 5, 1962, Ser. No. 185,303 6 Claims. (Cl. 73--423) This invention relates to automatic analysis apparatus and, more particularly, to sample supply means with which such apparatus is provided.

The object of the invention is to provide sample supply apparatus having a sample-liquid take-off tube in which provision is made for the introduction of air or other inert gas into the tube near its sample inlet end for dividing the flowing stream of sample liquid into segments of the liquid spaced from each other by intervening segments of the inert gas, whereby insoluble particulate matter which may be present in the liquid which is to be analyzed is prevented from settling out during the how of the liquid through the tubular conduits and other parts of the analysis apparatus. For example, but without limitation, when the analysis apparatus is used for the quantitative analysis of sewage or other Waste liquids in respect to known ingredients, the insoluble particulate matter which might be present in such liquids, whether or not the liquid is filtered, is prevented from settling out and contaminating the various conduits and other elements of the apparatus."

In the accompanying drawings which illustrate the presently preferred embodiment of the invention:

FIG. 1 is a more or less diagrammatic view of automatic analysis apparatus according to the present invention;

FIG. 2 is a view partly in elevation and partly in section showing part of the sample supply means, on an enlarged scale; and

FIG. 3 is an enlarged sectional view illustrating the segmentizing of the stream of sample liquid as soo as it enters the take-off tube. j

The analysis apparatus illustrated in FIG. 1 comprises the sample supply device which includes a carrier plate or support 12 for a series of removable cups or receptacles 14 which are supported in openings 16 of the plate by shoulders 18 of the cups as illustrated by FIG. 2. A take-off device 2% is mounted for pivotal movement on the pivot support indicated at 22 in FIG. 1, for movement of the take-off tube 24 into and out of the receptacles 14 for the flow of the sample liquids from the receptacles automatically for treatment for analysis and analysis after such treatment. The sample supply device It and its take-oil tube is advantageously of the construction shown and described in the US. Patent application of Jack Isreeli, Serial No. 666,403 filed June 18, 1957, now US. Patent No. 3,038,340 owned by my assignee. As described in said application, plate 12 is turned intermittently to bring the receptacles 14 in succession to the take-off station at which take-off tube 24 is located and said tube is pivotally moved about a horizontal axis into the receptacle and out of the receptacle while plate 12 isat rest. Alternatively, the take-off device may be mountedfor vertical up and down movement while the plate is at rest for the sample take-oit operation as disclosed in the US. application of De long, Serial No. 146,551, filed October 20, 1961 now US. Patent No. 3,134,263. Also, as shown in said De Jong application, the take-off device may be moved into and out of a receptacle which contains a wash liquid which is introduced thereby between successive samples.

During each rest period of plate 10, the sample liquid is aspirated from the receptacle by pump 26 which, as

here shown, includes a resiliently compressible tube 28 which is connected to the outlet end of take-off tube 24 as indicated at 39. Pump 26 is advantageously of the construction shown in my assignees US. Patent No. 2,935,028. As shown by said patent, the pump comprises a platen, herein indicated at 32, against which a plurality of resiliently compressible tubes are simultaneously compressed progressively along their lengths by spaced compression rollers, here indicated at 34, movable in an endless path longitudinally of said tubes by sprocket chains, here indicated at 36.

During the operation of the pump, a color developing reagent is introduced into the stream of sample liquid through pump tube 38 which is connected to tube at the fitting 40 from which the liquid flows to and through the mixing coil 42, which may be immersed in a heating bath (not shown) if desired or necessary to develop the color for colorimetric quantitative examina tion of the treated sample liquid in the colorimeter 4-4 in respect to a particular known ingredient. .The'colorimeter is of the continuous flow cell type and is operatively connected to a recorder 46 which provides a record of the quantitative analysis of each of the samples in succession in the stream of sample liquids during the operation of the apparatus. If a more detailed description of suitable automatic analysis apparatus is desired, reference may be had to the US. patent to Slreggs, No. 2,797,149, owned by the assignee of this application. It will be understood, however, that the analysis apparatus illustrated in FIG. 1 does not, per se, form part of my invention, except to the extent hereinafter indicated, and therefore does not requireimore detailed description, audit will be understood also that this invention does not relate to any particular method of chemical treatment but concerns generally a variety of well known analytical methods which therefore need not be particularly described.

In accordance with this invention, provision is made, as previously stated, for introducing air or any other inert gas into the take-01f tube 24 near its inlet end 48 (FIGS. 2 and 3). For this purpose, a tube 5% is secured to tube 24 and is in communication with the latter at the opening 52 as illustrated in FIG. 3. A pump tube 54 is connected to the inlet end of tube 50 as indicated at 56 in FIG. 1 so that during the operation of the pump, air under pressure is introduced into tube 55) and flows from the latter into tube 24 to segmentize the liquid as it flows through said tube; In FIG. 3, the liquid segments are indicated at L and are shown separated from each other by intervening segments of air indicated at A. Said air segments are operable to keep the fluid passages suliiciently clean to prevent contamination of one sample liquid by another sample liquid, as described in the above mentioned Skeggs patent, and are operable, pursuant to my present invention, to prevent settling out of particulate matter by reason of the introduction of the air into the take-off tube 24 substantially simultaneously with the flow of liquid from cup 14 into tube 24 by the operation of the pump-tube compression rollers on pump tubes 28 and 54.

It will be noted that air is pumped into tube 53 under pressure while the fluid is pumped through take-off tube 24 by the aspiration or suction efiect of pump tube 28. It will be understood that more fluid is pumped through tube 24 than is pumped into tube Sil. For this purpose pump tube 28 has a larger internal diameter than pump tube 54, the compression of said tubes along their lengths being effected simultaneously by the compression rollers. When take-0E device 26 is moved out of the receptacle only an is transmitted through tube 24 and this air is eliective to separate the samples from each other in pump tube 28. It will be understood that all of the air which is introduced into the take-off tube is removed, before the treated stream of sample liquid enters the part of the flow cell where it is exposed to the source of light in the colorimeter, so that the liquid segments are consolidated into a continuous liquid stream before it enters said part of the flow cell. For this purpose the inlet end of the fiow cell is vented, as shown for example in the above mentioned Skeggs patent.

While I have shown and described the presently preferred embodiment of my invention, it will be understood that the invention may be embodied in other ways and that in the illustrated embodiment certain changes may be made in the details of construction and in the form and arrangement of parts without departing from the underlying idea or principle of the invention within the scope of the appended claims.

What is claimed is:

1. Sample supply apparatus, comprising a receptacle for a sample liquid, a take-oh tube for the passage of a stream of liquid from said receptacle, said take-off tube being movable into and out of said receptacle and having an inlet for the liquid when said tube is in said receptacle, and means including a part in communication with said tube near said liquid inlet while said tube is in said receptacle for the introduction of an inert gas into said tube for dividing said liquid stream into a series of liquid segments spaced for each other by intervening segments of said gas, said part being movable with said take-oit tube into and out of said receptacle.

2. Sample supply apparatus, comprising a receptacle for a sample liquid, a take-cit tube for the passage of a stream of liquid from said receptacle, said take-elf tube being movable into and out of said receptacle and having an inlet for the liquid when said tube is in said receptacle, and tubular means including a part in communication with said tube near said liquid inlet while said tube is in said receptacle for the introduction of an inert gas into said'tube for dividing said liquid stream into a series of liquid segments spaced from each other by intervening segments of said gas, said part being movable with said take-oft tube into and out of said receptacle.

3. Sample supply apparatus, comprising a receptacle for a sample liquid, a take-ofi tube for the passage of a stream of liquid from said receptacle, said take-cit tube being movable into and out of said receptacle and having an inlet for the liquid when said tube is in said receptacle, means including a part in communication with said tube near said liquid inlet while said tube is in said receptacle for the introduction of an inert gas into said tube for dividing said liquid stream into a series of liquid segments spaced from each other by intervening segments of said gas said part being movable with said take-E tube into and out of said receptacle and pump means for supplying said inert gas under pressure to said tube and for simultaneously withdrawing for a sample liquid, a take-off tube for the passage of a stream of liquid from said receptacle, said take-off tube being movable into and out of said receptacle and having an inlet for the liquid when said tube is in said receptacle, tubular means including a part in communication with said tube near said liquid inlet while said tube is in said receptacle for the introduction of an inert gas into said tube for dividing said liquid stream into a series of liquid segments spaced from each other by intervening segments of said gas, said part being movable with said take-oif tube into and out of said receptacle and pump means for supplying said inert gas under pressure to said tubular means and for simultaneously aspirating the segmentized fluid stream from said takeoff tube.

5. Sample supply apparatus, comprising a receptacle for a sample liquid, a take-off tube for the passage of a stream of liquid from said receptacle, said take-otf tube being movable into and out of said receptacle and having an inlet for the liquid when said tube is in said receptacle, tubular means including a part in communication with said tube near said liquid inlet while said tube is said receptacle for the introduction of an inert gas into said tube for dividing said liquid stream into a series of liquid segments spaced from each other by intervening segments of said gas, said part being movable with said take-off tube into and out of said receptacle and pump means for supplying said inert gas under pressure to said tubular means and for simultaneously aspirating the segmentized fluid stream from said take- 01f tube at a higher flow rate than the flow rate of the inert gas through said tubular means.

d. Sample supply apparatus, comprising a receptacle for a sample liquid, a take-off tube for the passage of a stream of liquid from said receptacle, said take-off tube being movable into and out of said receptacle and having an inlet for the liquid when said tube is in said receptacle, means including a part in communication with said tube near said liquid inlet while said tube is in said receptacle for the introduction of an inert gas into said tube for dividing said liquid stream into a series of liquid segments spaced from each other by intervening segments of said gas, said part being movable with said take-oif tube into and out of said receptacle and pump means for supplying said inert gas under pressure to said tube and for simultaneously withdrawing the stream of fluid from said tube at a higher flow rate than the flovf rate of the inert gas into said tube.

References Cited by the Examiner UNITED STATES PATENTS 2,797,149 6/57 Skeggs.

2,879,141 3/59 Skeggs 73-424 X 2,899,280 8/59 Whitehead 23---- 253 X 2,946,665 7/60 Skeggs 23-253 X RICHARD C. QUEISSER, Primary Examiner.

ROBERT L. EVANS, Examiner, 

1. SAMPLE SUPPLY APPARATUS, COMPRISING A RECEPTACLE FOR A SAMPLE LIQUID, A TAKE-OFF TUBE FOR THE PASSAGE OF A STREAM OF LIQUID FROM SAID RECEPTACLE, SAID TAKE-OFF TUBE BEING MOVABLE INTO AND OUT OF SAID RECEPTACLE AND HAVING AN INLET FOR THE LIQUID WHEN SAID TUBE IS IN SAID RECEPTACLE, AND MEANS INCLUDING A PART IN COMMUNICATION WITH SAID TUBE NEAR SAID LIQUID INLET WHILE SAID TUBE IS IN SAID RECEPTACLE FOR THE INTRODUCTION OF AN INERT GAS INTO SAID TUBE FOR DIVIDING SAID LIQUID STREAM INTO A SERIES OF LIQUID SEGMENTS SPACED FOR EACH OTHER BY INTERVENING SEGMENTS OF SAID GAS, SAID PART BEING MOVABLE WITH SAID TAKE-OFF TUBE INTO AND OUT OF SAID RECEPTACLE. 